1-丁基-3-甲基咪唑六氟磷酸盐.doc

1-丁基-3-甲基咪唑六氟磷酸盐 离子液体合成研究 摘 要 离子液体是指完全由正负离子所组成并且在室温或接近室温下呈现液态的盐，也称为低温熔融盐。与传统的有机溶剂相比,它具有很多优点(1) 几乎没有蒸汽压、不挥发、无臭；(2) 有较大的稳定温度范围较好的化学稳定性及较宽的电化学窗口；(3) 通过阴阳离子的设计可调节其对水、有机物及聚合物的溶解性。 本实验通过微波辅助加热法制备1-丁基-3-甲基咪唑六氟磷酸盐离子液体。制备的基本过程：将药品l-甲基咪唑、溴代正丁烷、六氟磷酸钾按一定比例混合于反应容器内，然后置于微波炉中加热。将制得的产物进行提纯，并进行红外分析，确定其是否为目标产品。 本实验通过对加热方法、加热时间及药品的配比等方面的改变，最终确定一个产率较高的实验方案：将混合好的药品（l-甲基咪唑、溴代正丁烷、六氟磷酸钾摩尔比为：1:1.1:1.6）放入微波炉，功率调至最低，采用加热3 s，暂停30 s的间歇加热方法，反应时间100 min，再用去离子水和乙醚分别对其洗涤数次，最后对产物进行减压蒸馏，最终产物产率在60%左右。 关键词：微波，提纯，离子液体，红外光谱，1-丁基-3-甲基咪唑六氟磷酸盐 Study on synthesis of 1-BUTYL-3-METHYLIMIDAZOLIUM HEXAFLUOROPHOSPHATE IONIC LIQUID ABSTRACT? Ionic liquids are composed entirely of positive and negative ions, and present at or near room temperature liquid salt, also known as low-temperature molten salt. Compared with traditional organic solvents, it has many advantages: 1. almost no vapor pressure, non-volatile, colorless, odorless; 2. with a greater range of stable temperature, good chemical stability and wide?electrochemical interface; 3. it can be adjusted the solubility for water, organic compounds and polymers through the design of ions.  In this study, 1-butyl-3-methylimidazolium hexafluorophosphate ionic liquid was prepared using microwave.?The basic process of preparation: l-methylimidazole, n-butane bromide and potassium hexafluorophosphate were mixed in the container at a certain propotion, and then heated with the microwave. Purify the product, and take the infrared analysis to determine whether the target product.? The experimental program with a higher yield was ultimately established by changing heating method, heating time and the ratio of drugs and so on. Firstly, mixture of drugs were putted in the microwave ovens, most low-end gear prepared by heating 3 s, suspended?30 s intermittent heating method, reaction time was 100 min. Secondly, de-ionized water and ether were used to wash them several times, respectively. Finally, the products were carried on the reduced pressure d